CN105957706A - Method for preparing high-performance neodymium iron boron magnet by pressure impregnation of Dy<3+>/Tb<3+> - Google Patents

Method for preparing high-performance neodymium iron boron magnet by pressure impregnation of Dy<3+>/Tb<3+> Download PDF

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CN105957706A
CN105957706A CN201610274316.9A CN201610274316A CN105957706A CN 105957706 A CN105957706 A CN 105957706A CN 201610274316 A CN201610274316 A CN 201610274316A CN 105957706 A CN105957706 A CN 105957706A
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magnet
iron
neodymium
pressure
infiltration
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CN105957706B (en
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包小倩
卢克超
高学绪
李纪恒
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University of Science and Technology Beijing USTB
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered

Abstract

The invention discloses a method for preparing a high-performance neodymium iron boron magnet by pressure impregnation of Dy<3+>/Tb<3+>, and belongs to the field of a rare earth permanent magnetic material. The method comprises the specific technological steps of carrying out orientation compacting and vacuum pre-sintering on neodymium iron boron to obtain a partially-compacted pre-sintered blank; then dissolving a Dy/Tb salt into an organic solvent, and filtering the Dy/Tb salt organic solvent in the interior of the neodymium iron boron pre-sintered blank through a pressure impregnation way; keeping a part of the Dy<3+>/Tb<3+> in the interiors of the pre-sintered blank pores, and then further carrying out sintering densification to generate Dy<3+>/Tb<3+> grain boundary diffusion so as to improve the coercivity of the sintered neodymium iron boron magnet. The method has the advantages that the magnet is not limited by the dimensions and shapes; the diffusion path and the diffusion time of the Dy<3+>/Tb<3+> are greatly shortened; and high consistency in improvement of the internal organizational structure of the magnet and the improvement of the performance is realized.

Description

A kind of Pressure Infiltration Dy3+/Tb3+The method preparing high-performance neodymium-iron-boron magnet
Technical field
The invention belongs to field of rare-earth permanent magnetic, especially relate to a kind of Pressure Infiltration Dy3+/Tb3+Preparation The method of high-performance neodymium-iron-boron magnet.
Background technology
Sintered NdFeB magnet as third generation permanent magnet material, has the magnetic property of excellence, new-energy automobile, It is used widely in the fields such as wind-power electricity generation, medical apparatus and instruments, VCM, permanent magnetism high ferro.Due to rare earth permanent magnet material Expect, and the wasting of resources can be caused that the therefore application of high-end field is to promote to burn relatively thin in low side field profit The important motivity of knot neodymium iron boron industry development.High-end applications aspect is to the remanent magnetism Br of magnet, coercivity H i, magnetic Energy product (BH) max, squareness, heat-resistant stability and corrosion resisting property etc. all have higher requirement.Particularly burn The coercivity of knot neodymium iron boron magnetic body, less than theoretical value 30%, still has the biggest development space, and coercivity improves The heat-resistant stability of magnet, irreversible loss, squareness can be improved, therefore improve coercivity and become sintering neodymium The key of ferrum B permanent magnetic material development.
The coercivity of Sintered NdFeB magnet and microscopic structure have substantial connection, including Nd2Fe14B crystal grain The composition of (2:14:1 phase or principal phase), size, shape and border structure (crystal grain epitaxial layer, Grain-Boundary Phase Form, distribution etc.).By directly adding heavy rare earth element Dy/Tb during melting, replace principal phase Nd2Fe14Nd atom in B forms (Nd, the Dy/Tb) that anisotropy field is higher2Fe14B phase, is to improve magnet Coercivity is the most traditional and effective manner.But owing to the anti-ferromagnetism of heavy rare earth atom with Fe atom couples, Add too much heavy rare earth element and remanent magnetism and the magnetic energy product of magnet will necessarily be greatly lowered；And added multiple dilute Earth elements will necessarily improve production cost, is unfavorable for competition among enterprises, will also result in rare earth resources waste.Dual alloy Method and grain boundary decision technology are that research recent years is more can significantly improve the coercitive new technique of magnet, Magnet coercivity can be significantly improved, improve the utilization rate of heavy rare earth element, and less on remanent magnetism impact.
Grain boundary decision technology is more more efficient than dual alloy method, becomes the study hotspot of high-coercive force Sintered NdFeB magnet. Grain boundary decision technology be the neodymium iron boron magnetic body surface attachment one layer metal containing the heavy rare earth element such as Dy/Tb, Alloy or compound, be then passed through diffusion heat treatments, and heavy rare earth Dy/Tb enters magnet along magnet crystal boundary Inside, replaces Nd2Fe14The Nd atom of B Grain Surface forms the higher hard magnetized layer of magnetocrystalline anisotropy field, Thus improve the coercivity of magnet.Grain boundary diffusion process has obtained widely studied, and also there is numerous attachment side in diffusion source Formula, such as vapour deposition method (Wang Qingkai, Yu Yongjiang, Zhao Juntao, Li Yan, Li Guangjun, Ma Yukun. a kind of improve neodymium-iron-boron The coercitive device and method of power, CN102969110), sputtering method (Xu Feng, Chen Guang, Lu Guowen, Zhu Hainan, Lu Fengqi. the preparation method of a kind of low dysprosium content high performance sintered neodymium-iron-boron, CN102280240), surface be coated with Cover method (Luo Yang, sieve. grain boundary diffusion process for neodymium iron boron magnet, CN101845637), electrophoretic deposition (week Of heap of stone, Wang Lin, Li Jian, Yu Xiao army. the preparation method of rare earth permanent-magnetic material, CN102776547) etc..But these The adhering mode in diffusion source is often suitable only for thin slice magnet, and spreads source from magnet surface to the composition in magnet heart portion It is usually present Concentraton gradient, i.e. there is the inhomogeneities of bigger organizational structure and performance.
Summary of the invention
The invention aims to solve existing grain boundary decision Dy/Tb technology is only suitable for the thin slice that thickness is less Magnet, Dy/Tb diffusion needs longer path, and Dy/Tb concentration, with the inhomogeneities of magnet depth profile, is entered One step affects organizational structure and the problem of performance inhomogeneities.
A kind of Pressure Infiltration Dy3+/Tb3+The method preparing high-performance neodymium-iron-boron magnet, it is characterised in that soak with pressure The mode oozed is pre-at the neodymium iron boron of part fine and close (i.e. having certain porosity) by the organic solution of Dy/Tb salt In sintering briquette " filtration ", part Dy3+/Tb3+Stay in hole, then pass through sintering densification and Dy occurs3+/Tb3+ Grain boundary decision, thus improve the coercivity of sintered NdFeB.
Concrete technology step is as follows:
1) to neodymium iron boron pressed compact vacuum presintering, obtaining consistency is 65-95% (i.e. porosity 5-35%) Presintering base, and to surface cleaning process；
2) Dy/Tb salt is dissolved in organic solvent, obtains that there is the Dy that concentration is 0.1-5.0mol/l3+/Tb3+ Organic solution, Dy/Tb salt is (Dy/Tb) Cl3、(Dy/Tb)F3、(Dy/Tb)(NO3)3、(Dy/Tb)(ClO4)3、 (Dy/Tb)2(SO4)3、(Dy/Tb)2(SiO4)3At least one in Deng, organic solvent be ethanol, acetone, At least one in dichloromethane, dimethylformamide, dimethyl sulfoxide etc.；
3) being placed in infiltration jar by the neodymium iron boron presintered compact that part is fine and close, first evacuation, in utilizing tank, negative pressure sucks Dy3+/Tb3+Organic solution, and apply the gas pressure of 0.5-2.0MPa, make organic solution to neodymium iron boron Depths infiltration in presintered compact；
4) will be through Dy3+/Tb3+The presintering base that organic solution infiltrated is sintered densification and occurs Dy3+/Tb3+Grain boundary decision, temperature 900～1060 DEG C, the time 0.5～2h, pressure 0.3-10.0MPa (by Argon provides), applying argon gas initial vacuum degree (3-5) × 10-3Pa；
5) vacuum tempering is thermally treated resulting in high-coercive force Sintered NdFeB magnet, and technique is: temperature 450～650 DEG C, Time 1～4h, vacuum (3-5) × 10-3Pa。
The present invention utilizes pressure infiltration method will dissolve heavy rare earth Dy3+/Tb3+Organic solution be infiltrated up to have one Determining inside the neodymium iron boron presintered compact of porosity, the neodymium iron boron presintered compact with certain porosity is equivalent to porous material, Under pressure, heavy rare earth Dy has been dissolved3+/Tb3+Organic solution flow through with the form of " filtration " and have one When determining the neodymium iron boron presintering base of porosity, while there is " filtering flow ", neodymium iron boron presintered compact pair Dy3+/Tb3+" trapping " effect, part Dy can be produced3+/Tb3+Presintered compact internal void can be stayed, owing to being with molten The form of liquid filters, therefore Dy3+/Tb3+It is distributed visibly homogeneous in hole, makes through sintering further afterwards Presintering base is close to complete densification, and Dy occurs while sintering densification process3+/Tb3+Grain boundary decision, The surface layer of strengthening 2:14:1 crystal grain, thus improve coercivity.
It is an advantage of the current invention that:
1) magnet is not limited by size and dimension；
2)Dy3+/Tb3+Need the path of diffusion and be greatly shortened diffusion time；
3) concordance that magnet internal organizational structure is improved and performance improves is good.
Detailed description of the invention
Embodiment 1:
1) it is (NdPr) by composition30Fe68.7Cu0.1Zr0.2B1.0Orientation pressed compact at 1050 DEG C of vacuum presintering 1h, Obtain presintering base that consistency is 85% (porosity is 15%) (a size of), will The surface of presintering base is cleaned, numbered 1#；
2) by Dy (NO3)3·6H2O salt is dissolved in dimethylformamide, obtains the Dy that concentration is 0.3mol/l3+ Organic solution；
3) inserting in Pressure Infiltration tank by the presintered compact of numbered 1#, first evacuation, in utilizing tank, negative pressure sucks Dy3+/Tb3+Organic solution, and apply the gas pressure of 0.6MPa, make organic solution in neodymium iron boron presintered compact Depths is permeated, numbered 2#；
4) by 1# and 2# sample at same condition sintering densification, sintering temperature 1000 DEG C, time 1h, argon There is Dy in atmospheric pressure 2.0MPa, 2# sample sintering process simultaneously3+Grain boundary decision；
5) vacuum tempering heat treatment is carried out, tempering process: temperature 500 DEG C, time 2h, vacuum 3 × 10-3Pa；
6) NIM-2000 permanent magnetism is utilized to measure system test 1# and the magnetic property of 2# sample, performance parameter such as table 1 Shown in；Compared with 1#, after infiltration processes, the coercivity of 2# sample has had and has increased substantially, owing to passing through Infiltration processes, and the organic solution containing Heavy rare earth filters the hole of presintering base substrate equably, sinters and returns After fire process, tissue and the consistency of performance of magnet might as well.
The magnetic property of table 1 1# and 2# sample
Numbering Hci(kOe) Br(T) (BH)max(MGOe)
1# 13.5 1.445 50.5
2# 19.8 1.393 47.9
Embodiment 2:
1) it is (NdPr) by composition30Fe68.6Ga0.2Al0.2B1.0Orientation pressed compact at 1050 DEG C of vacuum presintering 1.5h, Obtain presintering base that consistency is 92% (porosity is 8%) (a size of), will be pre- The surface of sintered blank is cleaned, numbered 3#；
2) by Dy (NO3)3·6H2O salt is dissolved in dimethylformamide, obtains the Dy that concentration is 0.3mol/l3+ Organic solution；
3) inserting in Pressure Infiltration tank by the presintered compact of numbered 3#, first evacuation, in utilizing tank, negative pressure sucks Dy3+/Tb3+Organic solution, then applies the gas pressure of 0.8MPa, makes organic solution to neodymium iron boron presintered compact Interior depths is permeated, numbered 4#；
4) by numbered 3# and 4# sample in same condition sintering densification, sintering temperature 970 DEG C, time 1h, there is Dy in sintering process in argon pressure 4.0MPa, 4# sample simultaneously3+Grain boundary decision；
5) vacuum tempering heat treatment is carried out, tempering process: temperature 500 DEG C, time 2h, vacuum 3 × 10-3Pa；
6) NIM-2000 permanent magnetism is utilized to measure system test 3# and the magnetic property of 4# sample, performance parameter such as table 2 Shown in；Compared with 3#, after infiltration processes, the coercivity of 4# sample has had and has increased substantially, owing to passing through Infiltration processes, and the organic solution containing Heavy rare earth filters the hole of presintering base substrate equably, sinters and returns After fire process, tissue and the consistency of performance of magnet might as well.
The magnetic property of table 2 3# and 4# sample
Numbering Hci(kOe) Br(T) (BH)max(MGOe)
3# 13.7 1.441 50.3
4# 19.1 1.412 48.9

Claims (8)

1. a Pressure Infiltration Dy3+/Tb3+The method preparing high-performance neodymium-iron-boron magnet, it is characterised in that by pressure The mode of power infiltration by the organic solution of Dy/Tb salt in the fine and close neodymium iron boron presintered compact of part " filtration ", portion Divide Dy3+/Tb3+Stay in presintered compact hole, then pass through sintering densification and Dy occurs3+/Tb3+Grain boundary decision, Thus improve the coercivity of sintered NdFeB；
Concrete technology step is as follows:
1) neodymium iron boron is orientated pressed compact vacuum presintering, obtains the presintered compact that part is fine and close, i.e. have certain porosity, And surface cleaning is processed；
2) Dy/Tb salt is dissolved in organic solvent, obtains that there is certain density Dy3+/Tb3+Organic solution；
3) by Dy by the way of vacuum pressure infiltration3+/Tb3+Organic solution is infiltrated up to presintered compact internal void；
4) through Dy3+/Tb3+The further sintering densification of presintered compact that organic solution infiltrated also occurs Dy3+/Tb3+Grain boundary decision；
5) vacuum tempering is thermally treated resulting in high-coercive force Sintered NdFeB magnet.
2. a kind of Pressure Infiltration Dy3+/Tb3+The method preparing high-performance neodymium-iron-boron magnet, It is characterized in that processing step 1) in the consistency of presintered compact require as 65-95%, i.e. porosity 5-35%.
3. a kind of Pressure Infiltration Dy3+/Tb3+The method preparing high-performance neodymium-iron-boron magnet, It is characterized in that processing step 2) in Dy/Tb salt be: (Dy/Tb) Cl3、(Dy/Tb)F3、(Dy/Tb)(NO3)3、 (Dy/Tb)(ClO4)3、(Dy/Tb)2(SO4)3、(Dy/Tb)2(SiO4)3In at least one, Dy/Tb can be independent Or associating compatibility.
4. a kind of Pressure Infiltration Dy3+/Tb3+The method preparing high-performance neodymium-iron-boron magnet, It is characterized in that processing step 2) in organic solvent be: ethanol, acetone, dichloromethane, dimethylformamide, At least one in dimethyl sulfoxide organic solvent.
5. a kind of Pressure Infiltration Dy3+/Tb3+The method preparing high-performance neodymium-iron-boron magnet, It is characterized in that processing step 2) in Dy3+/Tb3+The concentration of organic solution is 0.1-5.0mol/l.
6. a kind of Pressure Infiltration Dy3+/Tb3+The method preparing high-performance neodymium-iron-boron magnet, It is characterized in that processing step 2) in neodymium iron boron presintered compact be placed in infiltration jar, first evacuation, negative in utilizing tank Pressure sucks Dy3+/Tb3+Organic solution, then applies the gas pressure of 0.5-2.0MPa, make organic solution to Depths infiltration in neodymium iron boron presintered compact.
7. a kind of Pressure Infiltration Dy3+/Tb3+The method preparing high-performance neodymium-iron-boron magnet, It is characterized in that processing step 4) in sintering process be: sintering temperature 900～1060 DEG C, the time 0.5～2h, Argon pressure 0.3-10.0MPa, applying argon gas initial vacuum degree (3-5) × 10-3Pa。
8. a kind of Pressure Infiltration Dy3+/Tb3+The method preparing high-performance neodymium-iron-boron magnet, It is characterized in that processing step 5) in vacuum tempering technique be: temperature 450～650 DEG C, the time 1～4h, very Reciprocal of duty cycle (3-5) × 10-3Pa。
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CN106782973A (en) * 2016-12-14 2017-05-31 安徽大地熊新材料股份有限公司 A kind of preparation method of anti-corrosion Sintered NdFeB magnet high
CN107617737A (en) * 2017-11-10 2018-01-23 湖南稀土金属材料研究院 Sintered Nd-Fe-B permanent magnetic material powder and its preparation method and application
CN109003799A (en) * 2018-07-06 2018-12-14 杭州永磁集团振泽磁业有限公司 A kind of preparation method of high-coercive force neodymium iron boron magnetic body
CN109935462A (en) * 2019-03-12 2019-06-25 宁波雄海稀土速凝技术有限公司 The preparation method and its neodymium iron boron magnetic body of grain boundary decision heavy rare earth neodymium iron boron magnetic body
CN110556243A (en) * 2019-08-19 2019-12-10 安徽省瀚海新材料股份有限公司 neodymium iron boron surface dysprosium penetration method
CN113889336A (en) * 2021-12-08 2022-01-04 天津三环乐喜新材料有限公司 Preparation method of high-performance neodymium iron boron permanent magnet
CN115206665A (en) * 2022-09-14 2022-10-18 宁波科宁达工业有限公司 Neodymium-iron-boron permanent magnet and preparation method thereof

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CN106782973A (en) * 2016-12-14 2017-05-31 安徽大地熊新材料股份有限公司 A kind of preparation method of anti-corrosion Sintered NdFeB magnet high
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CN110556243B (en) * 2019-08-19 2021-07-02 安徽省瀚海新材料股份有限公司 Neodymium iron boron surface dysprosium penetration method
CN113889336A (en) * 2021-12-08 2022-01-04 天津三环乐喜新材料有限公司 Preparation method of high-performance neodymium iron boron permanent magnet
CN113889336B (en) * 2021-12-08 2022-03-11 天津三环乐喜新材料有限公司 Preparation method of high-performance neodymium iron boron permanent magnet
CN115206665A (en) * 2022-09-14 2022-10-18 宁波科宁达工业有限公司 Neodymium-iron-boron permanent magnet and preparation method thereof

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